Abstract
Well-crystallized Li4Mn5O12powder was prepared by heating a eutectic mixture of lithium acetate LiOAc and manganese nitrate Mn(NO3)2in an O2atmosphere. The structure of Li4Mn5O12crystallites was found to be cubic spinel using Rietveld refinement of both neutron and X-ray powder diffraction profiles. We confirmed that lithium ions occupy both the tetrahedral sites 8aand part of the octahedral sites 16d, but not the 16csites in the space groupFd3m, while all the manganese ions occupy the 16dsites. The lattice parameter was found to be sensitive to synthesis temperature as a result of the variation in manganese valence. The presence of Mn3+leads to the formation of a stoichiometric spinel Li[LixMn2−x]O4in whichxdecreases from 1/3 (Li4Mn5O12) to 0 (LiMn2O4), with concomitant formation of Li2MnO3depending on the synthesis conditions.
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